Process and apparatus for splitting coal, oils, and other hydrocarbons



March 12, 1929. A. DEBO 1,704,792

PROCESS AND APPARATUS FOR SPLITTING COAL, OILS, AND OTHER HYDROCARBONS Filed May 15, 1925 removed again Patented Mar. 12, 1929.

ARNO DEBO, OF MANNHEIM-RHEINAU, BERGIN-COMPAGNIE VOOR OLIE-EN LANDS.

GERMANY, ASSIGNOR TO INTERNATIONALE KOLEN-CHEMIE, OF THE HAGUE, NETHER- PROCESS AND APPARATUS FOR SPLITTING COAL, OILS, AND OTHER HYDROCARBONS.

Application filed May 15, 1925, Serial No. 30,555, and in Germany May 23, 1924.

It is already known that it is possible to hydrogenate and split coal, oils, and other heavy hydrocarbons so as to from readily volatile liquid products, such as benzinc, petroleum and the like,

obtain thereby highly heating the initial materials with hydrogen under high pressure and condensing the products ber pressures distilled olf. In the reaction chamof 100 to 150 atmospheres and even more, and a temperature of about 300 to 500 C. prevail.

If solid raw materials,

such as coal, are

be, the more fully is the capa city of the reaction vessel utilized. If liquid substances,

such as mineral oils or other are to be hydrogenated an substances are added thereto sorption mediaand the like,

shales or the like, for the purpose such as diatomite, or alkaline earth oxides, oil

hydrocarbons, d split, solid for example coke ashes of preventing deposition and burning of asphaltic materials and separation of coke.

Thus in all cases there is the problem of forcing a mixture of solid and vessel in which a very liquid substances into a high pressure prevails.

If the hydrogenating and splitting of the initial materials in the reaction chamber has taken place in the presence of hydrogen, the

reaction products must then be continuously from the high-pressure vessel. These products are condensable and noncondensable gases on and solid residues on the 0th separation thereof has hithert by drawing off highest point 0 the one hand and liquid er hand. The 0 been effected the gaseous products from the f the heated receptacles while the residues are drawn off at the lowest point. Certain disadvantages and (llll'lCllltlQS are connected with this procedure A special difficulty with the method of working hitherto employed consists in the uncertainty of maintaining a level in the closed high-pressure cont definite liquid ainer,

the interior is not accessible to observation.

If the filling becomes too grea t, the action of the hydrogen is level sinks too 10 burnt.

incomplete. If the liquid w, the mass is liable to be Now the present invention relates to a new process for forcin the solid and liquid raw materials into the igh-pressure vessel in the form of paste, and withdrawing the gaseous,

solid and liquid products of reaction continuously from the high-pressure container in such a manner that a definite liquid level is always maintained in the interior of the container.

While the pumping in of thick liquids, even in the case of the abovementioned high pressures, hardly causes any difficulties, paste-like masses, which are no longer fluid cannot be forced into high-pressure vessels on a large scale Without special precautions. the thicker the mass is, the larger must be the suction aperture of the press or pump, and in the case of stiff pastes it must be so large that the clearance spaces would assume excessive dimension s, as a result of which. the

useful effect attainable would be very considerably impaired.

This difiiculty has hitherto been met by conveying such pastes by means of liquids under pressure. Ev

en then however a mixture could not be made as thick as would be desirable because otherwise the liquid under pressure would penetrate into the stiff mass instead of driving the latter before it. On this account. when forcing in a coal paste, it was not possible to take more than 1.4 parts of pulverized coal to 1 part of oil.

According to the present invention these difiiculties are removed by first compressing the mass to be forced into a low pressure, and then immediately further pressing into the retort under a high pressure.

The elimination of the compressed liquid now makes it possible to convey coal to one part pressure is prefer worm conveyor.

2 to 2.5 parts of powdered of oil. This preliminary ably effected by means of a \Vhen working without such preliminary compression only a pressure of 1 atmosphere can be used for filling the pump chamber but now a pressure of 3 to 5 atmospheres for example can be used. This combination of a high-pressure press with a worm conveyor therefore presents special advantages, because b means of the latter it is immediately possible to make the inlet apertures as large as may be desired, while on the other hand the disadvantage of such a Worm conveyor namely its unfavorable mechanical efliciency, is not important, as out of the total pressure drop of, say, 150 atmospheres, only from 3 to 5 atmospheres, that is to say, onefiftieth to one-thirtieth of the whole, is affected by this low efficiency, while by far the greater part of the work done is carried out in the cylinder of a press at high efficiency.

While provision is made in this manner for the continuous and certain supplying of the raw materials to the high-pressure container, the removal of the products of reaction at the other end of the reaction container is also effected in such a manner that no dangerous sinking of the surface level of the liquid can take place. For this purpose, no separate removal of the gaseous and of the liquid and solid reaction products takes place, but the whole mixture is drawn off together from the container, this being done at a position located between the highest and lowest points, for example through a dipping pipe which extends down to the level of the normal surface of the liquid. In order to be able to draw off the constituents in all three states of aggregation together at such a position, a thorough mixing up of the entire contents of the container is indispensable. Stirring would however in any case have to be resorted to in order to prevent any settling out and on account of the fundamental mixing. In View of the distinctive character of the hydrogenation a large contact surface must be presented to the hydrogen and a definite duration of the action must be allowed. That is also the reason Why the. withdrawal of all the constituents, including the excess hydrogen. should not take place at the top of the vessel.

The carrying out of the process will now be explained in reference to the accompanying drawing. In this drawing 1 denotes a worm conveyor provided with a bunker or hopper 2. which forces the paste to be supplied to a high-pressure vessel 12 into a pipe 3. The latter leads through valves 4 and 5 to a press cylinder 6, in which a piston 7 is reciprocated under the act-ion of a hydraulic driving mechanism 8, also constructed as a press cylinder. By the motion of the piston 7 the paste forced into the cylinder is forced through further valves 9 and 10 into a pipe 11, which is conlfiegted with the high-pressure vessel 12 to be The necessary hydrogen is continuously pumped in by a pump 13. The reaction vessel 12 is provided with stirring mechanism having driving means 14, the object of which is to prevent the deposition of solid materials and thoroughly to mix up the gaseous, liquid and solid substances that are to take part in the reaction. At the same time the stirring mechanism may also serve by suitable means to prevent mixing up in the longitudinal direction of the reaction vessel, and thereby en sure a sufficiently long duration for the reaction. Such means are for example the discs 15 fitted on to the stirrer, which extend almost throughout the cross section of the vessel, leaving only a narrow gap at the periphcry.

The substances taking part in the reaction and the products arising therefrom flow gradually through the reaction chamber in its longitudinal direction and in this manner arrive at the outlet aperture, which is formed as an immersed or dip pipe 16 and through a pipe connected thereto and a throttle valve 17 into a collecting passage 18, in which separation of the liquid and solid products from the gaseous products takes place at atmospheric pressure. While the gases are flowing through a pipe 20 to a gasometer the liquid and solid parts are drawn off from time to time through a valve 21. The throttle valve 17 is so adjusted that the pressure in the reaction chamber, indicated on a pressure gauge 22, remains constant throughout the Whole duration of the operation.

In the case of the process described, the liquid level in the reaction vessel remains constantly adjusted to the height of the discharge aperture. If from any cause it falls somewhat lower, as a result for example of a temporary disturbance of the pump 7, no idle running and burning can occur, because gas is only drawn off from the pipe 16 until liquid level rises again. If the dip tube 16 begins to become immersed in the liquid, a rise of pressure occurs in the apparatus owing to the new products produced, and this rise of pressure is indicated by the pressure gauge 22. This pressure is then reduced again by regulating the throttle valve 17, and the surface level of the liquid sinks back to the mouth of the dipping tube.

In addition to the advantages already indicated it may be mentioned that the separating of the individual reaction products after expansion to atmospheric pressure is even simpler, easier and more complete than in the high pressure vessel, as hitherto arranged.

What I claim is 1. A process for maintaining continuously a definite liquid level in the interior of a high-pressure chamber when splitting coal, oils and other hydrocarbons by heating these initial materials with hydrogen at a high pressure, consisting in converting said materials into a paste-like mass, compressing said paste-like mass to a pressure of a few atmospheres, and then forcing it into the highpressure chamber, and subsequently drawing off the gaseous, liquid and solid products of reaction together from said high-pressure the compressed paste like mass into the high container at a point located between the highpressure chamber a tube in the high-pressure est and lowest parts thereof. chamber which dips down to a point inter- 2. An apparatus for maintaining a definite mediate the highest and lowest points thereof 5 liquid level in the interior of a high pressure for drawing off the solid, liquid, and gaseous chamber when splitting coal, oils and other reaction products together. hydrocarbons by heating with hydrogen at a In testimony whereof I have signed my high pressure comprising a worm conveyer name to this specification. for compressing a paste-like mass to a pres- 10 sure of a few atmospheres, a pump for forcing ARNO DEBO. 

